双波长分光光度法测定食盐中硒含量

在聚乙烯醇(PVA)存在下,在pH10.4的NaHCO3-NaOH缓冲溶液中,硒(IV)与1-(2-吡啶偶氮)-2-萘酚(PAN)、溴化十六烷基吡啶(CPB)反应形成稳定的络合物,该络合物在410 nm处有正吸收峰,529 nm处有负吸收峰,据此建立了双波长光度法测定痕量硒(IV)的新方法。硒(IV)浓度在0~0.12μg/mL内符合比尔定律,方法检出限为1.82μg/L,表观摩尔吸光系数ε为3.38×105L.mol-1.cm-1。方法用于硒强化营养盐和健康平衡盐中硒含量的测定,结果与荧光法测定值一致,相对标准偏差为0.82%~1.16%(n=5),加标回收率为99.7%~101.0%。     

1-(2-吡啶偶氮)-2-萘酚光度法测定蕨菜中痕量锌的研究

研究了用Zn2 -1-(2-吡啶偶氮)-2-萘酚分光光度法测定蕨菜中痕量锌的最佳条件。其表观摩尔吸光系数为1.42×104L/mol·cm,Zn2 含量在0～100μg/50mL范围服从比尔定律,检测限为0.5μg/dm3。相对标准偏差在1.3%～2.1%,回收率在98%～103%。测得结果与用原子吸收法验证的结果非常吻合,法准确度和精密度均较好,操作简便、快速、该法可用于蕨科草本植物中痕量锌的快速测定。     

高灵敏度分光光度法测定饲料中牛磺酸含量

采用盐酸浸提和离子交换法对饲料前处理,根据痕量牛磺酸在pH 11.0氨-氯化铵缓冲溶液中能抑制高锰酸钾氧化氨基黑10B的反应,使体系吸光度明显减小,建立了高灵敏度分光光度法测定饲料中牛磺酸的新方法。试验了酸度、高锰酸钾用量、氨基黑10B用量、反应温度和时间对测定的影响,确定了最佳反应条件,还考察了共存物质对测定的干扰情况。在优化的反应条件下,最大褪色波长位于620 nm,体系褪色程度与牛磺酸质量浓度在0~100 μg/L范围内呈良好的线性关系,相关系数为0.9995,表观摩尔吸光系数为5.82×105 L.mol-1.cm-1,检出限为3.5 μg/L。将该法用于饲料中牛磺酸的测定,相对标准偏差为0.98%~1.29%,回收率为97.2%~102.7%。该方法灵敏、准确、简便、快速、精密度高,选择性好,反应条件温和,对环境友好,完全满足饲料中牛磺酸含量的检测要求。     

2-(2-氰基-4-硝基-6-溴苯偶氮)对苯二酚分光光度法测定食品中铅

目的:探索测定食品中痕量铅的新方法.方法:以新试剂2-(2-氰基-4-硝基-6-溴苯偶氮)对苯二酚作为显色剂,研究分光光度法测定铅的优化条件.结果:在HArNaAc缓冲溶液中,铅(Ⅱ)与显色剂形成桔红色络合物,最大吸收波长为457 nm,表观摩尔吸光系数ε=5.13×104 L·mol-1·cm-1,铅的质量在0-15 μg/25 mL范围内符合比耳定律.相对标准偏差为2.3%-2.8%.结论:该方法准确度、精密度良好,是一种简便、可靠的测定食品中铅的方法.     

纸层析-酶标仪法测定发酵液中γ-氨基丁酸

建立纸层析-酶标仪法对微孔板发酵液中γ-氨基丁酸产量进行测定。对影响纸层析-酶标仪法测定结果的重要因素进行优化,并建立相应的分光光度法。优化后层析液中显色剂-茚三酮的浓度为8 g/L,展开剂-正丁醇、冰醋酸与水3者体积比为2∶1∶1;洗脱液中乙醇的体积分数为75%,乙醇与质量浓度为6 g/L CuSO_4·5H_2O的体积比为39∶1;γ-氨基丁酸质量浓度在1～7 g/L之间,吸光度与样品浓度线性关系良好(R~2=0. 999 0),平均回收率为98. 248 5%,重复性RSD为2. 625 5%。纸层析-酶标仪法能快速、准确地测定微孔板发酵液中γ-氨基丁酸产量,为后续高通量选育γ-氨基丁酸高产菌株奠定了基础。     

磺胺-氨基萘磺酸光度法测定食品中亚硝酸盐

筛选了重氮组分和偶合组分.研究了重氮反应和偶合显色反应的条件和方法,提出了磺胺-8-氨基-1-萘磺酸分光光度法测定食品中亚硝酸盐.常温,溴化钾共存下,亚硝酸盐在 pH 3的磷酸-磷酸二氢钠缓冲溶液中与磺胺发生重氮化反应,重氮盐与8-氨基-1-萘磺酸偶合生成红色偶氮化合物,最大吸收峰在518 nm波长处.磺胺-8-氨基-1-萘磺酸偶氮化合物的表观摩尔吸光系数 3.9×104 L·mol-1·cm-1,线性范围0.02～1.4 mg/L,相对标准偏差2.22%,回收率98.0%～102%.该方法可用于食品中痕量亚硝酸盐的测定.     

乙醇体系中酶抑制法检测氨基甲酸乙酯的研究

研究了在乙醇-水溶液和乙醇-缓冲液体系中,以乙酰胆碱酯酶对底物碘化硫代乙酰胆碱进行水解。根据氨基甲酸乙酯对乙酰胆碱酯酶的抑制率与吸光度的线性关系,测定体系中氨基甲酸乙酯的含量。实验发现,在乙醇-水溶液中,此方法不可行;而在低浓度乙醇-缓冲液体系中,氨基甲酸乙酯对乙酰胆碱酯酶的抑制率与其浓度在一定范围内呈线性关系。在5%、10%和15%乙醇-缓冲液体系中测定氨基甲酸乙酯的线性范围分别为2~10、1~5、1~5mg/L,相关系数在0.992~0.997之间,最低检出限为0.00895、0.04259、0.02916mg/L,RSD分别在1.41%~2.17%、0.34%~0.55%和3.61%~6.44%范围内。该法快速简便,所用仪器设备简单,检测成本低。本研究为酒精饮料及发酵食品中氨基甲酸乙酯的快速、简便、低成本检测方法的研究及相关产品的开发提供一定的理论和数据支持。     

分光光度法测定食品中的铝含量

依据国家标准方法[1]对样品的前处理和样品的测定进行研究.样品前处理采用干灰化法.在pH 6.0的乙酸-乙酸钠缓冲介质中,铝在聚乙二醇辛基苯醚(OP)和溴化十六烷基三甲胺的存在下与铬天青S形成稳定的四元混合胶束体系,其吸光度与铝含量在一定浓度范围内成正比.结果:摩尔吸光系数为7.1×10 4 L/mol·cm.铝含量在0.00～5.00 μg/25 mL呈良好的线性关系,相关系数r=0.9995,回收率在95.8%～99.8%之间.该法操作简单,显色灵敏、稳定、精密度和准确度高,适用于各种食品中铝含量测定的要求.     

C18色谱柱去除3-氯-1,2-丙二醇酯测定中的干扰组分

为了在油脂3-氯-1,2-丙二醇酯含量测定中通过预分离过程去除干扰组分,研究对比了固相萃取柱与硅胶柱层析对油样的分离效果。结果表明:油样的乙腈提取液用SunFireTMC18色谱柱(4.6mm×150 mm,5μm)分离,以乙腈-异丙醇(体积比1∶1)为流动相,等度洗脱,柱温30℃,流速1 mL/min的HPLC条件下,可以将不同极性的组分进行分离,从而有效去除3-氯-1,2-丙二醇酯测定中的干扰组分。在自制油样中分别添加800、1 000 mg/kg和1 200 mg/kg的3-氯-1,2-丙二醇酯标准品进行加标回收试验,1,2-二油酸酰-3-氯丙二醇的加标回收率在86.4%~113.7%,1-硬脂酰-3-氯丙二醇的加标回收率在88.4%~105.6%,相对标准偏差均在15%以内。该法耗用溶剂量少且周期较短,可用于大量样本3-氯-1,2-丙二醇酯测定中干扰组分的去除。     

1-(2-吡啶偶氮)-2-萘酚光度法测定人发中微量钴

钴是人体内重要的微量元素,也是人体健康状况的指标之一。在Tween-80存在下,pH5的缓冲溶液中,1-(2-吡啶偶氮)-2-萘酚可以和钴结合形成络合物,该络合物体系性质稳定,显色灵敏,其最大吸收波长580 nm,摩尔吸光系数3.65×104L.mol-1.cm-1,线性范围0～12μg/mL。本研究实测了人发样品中钴含量并与原子吸收法做对比试验,RSD(n=6)为1.7-3.0%,回收率95.1-101.5%,建立了一种适于普通医疗机构临床检测的灵敏、方便、实用的钴含量分析技术,该技术可用于临床医疗检测。     

Reliable identification of grapevine rootstock varieties using RAPD PCR on woody samples

Since grapevine ( Vitis spp .) rootstock material is being traded increasingly as disbudded woody material a lack of distinctive morphological features on such material necessitates an alternative and reliable means of identification. Methods described here were developed for rapid and efficient extraction of DNA from woody samples rich in phenolic compounds and polysaccharides, and for subsequent identification of varieties by RAPD PCR. Using these methods, and with the application of only one selected RAPD primer, we were able to differentiate sixteen rootstock varieties, including the seven varieties most commonly used in Germany. Problems commonly encountered with reproducibility of RAPD patterns were avoided by choosing primers with a dinucleotide sequence and a high G/C content that allowed a rather high annealing temperature of 45°C. Methods described here should also be useful for other horticultural crops, especially those with woody tissues rich in phenolic compounds and polysaccharides.     

An internet compendium of analytical methods and spectroscopic information for monomers and additives used in food packaging plastics

An internet website (http://cpf.jrc.it/smt/) has been produced as a means of dissemination of methods of analysis and supporting spectroscopic information on monomers and additives used for food contact materials (principally packaging). The site which is aimed primarily at assisting food control laboratories in the European Union contains analytical information on monomers, starting substances and additives used in the manufacture of plastics materials. A searchable index is provided giving PM and CAS numbers for each of 255 substances. For each substance a data sheet gives regulatory information, chemical structures, physico-chemical information and background information on the use of the substance in particular plastics, and the food packaging applications. For monomers and starting substances (155 compounds) the infra-red and mass spectra are provided, and for additives (100 compounds); additionally proton NMR are available for about 50% of the entries. Where analytical methods have been developed for determining these substances as residual amounts in plastics or as trace amounts in food simulants these methods are also on the website. All information is provided in portable document file (PDF) format which means that high quality copies can be readily printed, using freely available Adobe Acrobat Reader software. The website will in future be maintained and up-dated by the European Commission's Joint Research Centre (JRC) as new substances are authorized for use by the European Commission (DG-ENTR formerly DGIII). Where analytical laboratories (food control or other) require reference substances these can be obtained free-ofcharge from a reference collection housed at the JRC and maintained in conjunction with this website compendium.     

Aroma characterization of various apricot varieties using headspace–solid phase microextraction combined with gas chromatography–mass spectrometry and gas chromatography–olfactometry

The characterization of the aromatic profile of several apricot cultivars with molecular tracers in order to obtain objective data concerning the aromatic quality of this fruit was undertaken using headspace–solid phase microextraction (HS–SPME). Six apricot cultivars were selected according to their organoleptic characteristics: Iranien, Orangered, Goldrich, Hargrand, Rouge du Roussillon and A4025. The aromatic intensity of these varieties measured by HS–SPME–Olfactometry were defined and classified according to the presence and the intensity of grassy, fruity and apricot like notes. In the six varieties, 23 common volatile compounds were identified by HS–SPME–GC–MS. Finally, 10 compounds, ethyl acetate, hexyl acetate, limonene, β-cyclocitral, γ-decalactone, 6-methyl-5-hepten-2-one, linalool, β-ionone, menthone and (E)-hexen-2-al were recognized by HS–SPME–GC–O as responsible of the aromatic notes involved in apricot aroma and considered as molecular tracers of apricot aromatic quality which could be utilized to discriminate apricot varieties.     

Tests of potential functional barriers for laminated multilayer food packages. Part I: Low molecular weight permeants

The advent of the functional barrier concept in food packaging has brought with it a requirement for fast tests of permeation through potential barrier materials. In such tests it would be convenient for both foodstuffs and materials below the functional barrier (sub-barrier materials) to be represented by standard simulants. By means of inverse gas chromatography, liquid paraffin spiked with appropriate permeants was considered as a potential simulant of sub-barrier materials based on polypropylene (PP) or similar polyolefins. Experiments were performed to characterize the kinetics of the permeation of low molecular weight model permeants (octene, toluene and isopropanol) from liquid paraffin, through a surrogate potential functional barrier (25 μm-thick oriented PP) into the food simulants olive oil and 3% (w/v) acetic acid. These permeation results were interpreted in terms of three permeation kinetic models regarding the solubility of a particular model permeant in the post-barrier medium (i.e. the food simulant). The results obtained justify the development and evaluation of liquid sub-barrier simulants that would allow flexible yet rigorous testing of new laminated multilayer packaging materials.     

Chlorohydrins of bisphenol A diglycidyl ether (BADGE) and of bisphenol F diglycidyl ether (BFDGE) in canned foods and ready-to-drink coffees from the Japanese market

BADGE.2HCl and BFDGE.2HCl were determined in 28 samples of ready-to-drink canned coffee and 18 samples of canned vegetables (10 corn, 5 tomatoes and 3 others), all from the Japanese market. HPLC was used as the principal analytical method and GCMS for confirmation of relevant LC fractions. BADGE.2HCl was found to be present in one canned coffee and five samples of corn, BFDGE.2HCl in four samples of canned tomatoes and in one canned corn. No sample was found which exceeded the 1mg/kg limit of the EU for the BADGE chlorohydrins. However the highest concentration was found for the sum of BFDGE.2HCl and BFDGE.HCl.H₂O at a level of 1.5mg/kg. A Beilstein test confirmed that all cans containing foods contaminated with BADGE.2HCl or BFDGE.2HCl had at lest one part coated with a PVC organosol.     

European priorities for research to support legislation in the area of food contact materials and articles

A strong science base is required to underpin the planning and decision-making process involved in determining future European community legislation on materials and articles in contact with food. Significant progress has been made in the past 5 years in European funded work in this area, with many developments contributing to a much better understanding of the migration process, and better and simpler approaches to food control. In this paper this progress is reviewed against previously identified work-areas (identified in 1994) and conclusions are reached about future requirements for R&D to support legislation on food contact materials and articles over the next 5 or so years.     

Analysis of benzo[a]pyrene in spiked fatty foods by second derivative synchronous spectrofluorimetry after microwave-assisted treatment of samples

A simple, rapid and inexpensive method has been developed for the determination of benzo[a     

The development of reference materials for paralytic shellfish poisoning toxins in lyophilized mussel. II: Certification study

This paper describes the second part of a project undertaken to develop certified mussel reference materials for paralytic shellfish poisoning toxins. In the first part two interlaboratory studies were undertaken to investigate the performance of the analytical methodology for several PSP toxins, in particular saxitoxin and decarbamoyl-saxitoxin in lyophilized mussels, and to set criteria for the acceptance of results to be applied during the certification exercise. Fifteen laboratories participated in this certification study and were asked to measure saxitoxin and decarbamoyl-saxitoxin in rehydrated lyophilized mussel material and in a saxitoxin-enriched mussel material. The participants were allowed to use a method of their choice but with an extraction procedure to be strictly followed. The study included extra experiments to verify the detection limits for both saxitoxin and decarbamoyl-saxitoxin. Most participants (13 of 15) were able to meet all the criteria set for the certification study. Results for saxitoxin.2HCl yielded a certified mass fraction of <0.07 mg/kg in the rehydrated lyophilized mussels. Results obtained for decarbamoyl-saxitoxin.2HCl yielded a certified mass fraction of 1.59+/-0.20 mg/kg. The results for saxitoxin.2HCl in enriched blank mussel yielded a certified mass fraction of 0.48 +/- 0.06 mg/kg. These certified reference materials for paralytic shellfish poisoning toxins in lyophilized mussel material are the first available for laboratories to test their method for accuracy and performance.     

Announcing a new international peer-reviewed journal:Food Science and Human Wellness now accepting manuscript submission in English

<正>We are pleased to announce the launch of a new international peer-reviewed journal-Food Science and Human Wellness,ISSN 2213-4530,which is an open access journal,produced and hosted by Elsevier B.V.on behalf of Beijing Academy of Food Sciences.Food Science and Human Wellness is an international peer-reviewed English journal that provides a forum for the dissemination of the